++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04mbh0606 started at 14:13:57 on 28-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.865 9.416 19.127 98.13 95.13 97.98 15112 Reflections read from file 04mbh0606.hkl; mean (I/sigma) = 4.91 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7535 7580 7553 7558 11334 10087 10076 15112 N (int>3sigma) = 0 3451 3494 3461 3438 5203 4594 4628 6851 Mean intensity = 0.0 191.4 181.9 188.7 194.1 187.3 194.5 190.0 186.7 Mean int/sigma = 0.0 5.1 5.1 5.1 5.1 5.1 5.1 5.1 5.0 Lattice type: P chosen Volume: 853.69 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 4.865 9.416 19.127 98.13 95.13 97.98 Niggli form: a.a = 23.67 b.b = 88.66 c.c = 365.86 b.c = -25.48 a.c = -8.31 a.b = -6.36 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.092 [ 11174] Cell: 4.865 9.416 19.127 98.13 95.13 97.98 Volume: 853.69 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7535 7580 7553 7558 11334 10087 10076 15112 N (int>3sigma) = 0 3451 3494 3461 3438 5203 4594 4628 6851 Mean intensity = 0.0 191.4 181.9 188.7 194.1 187.3 194.5 190.0 186.7 Mean int/sigma = 0.0 5.1 5.1 5.1 5.1 5.1 5.1 5.1 5.0 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.924 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.092 11174 0.0 / 5.0 2.20 [B] P1 # 1 chiral 1 700 0.092 11174 0.0 / 5.0 5.66 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C4 H6 O6 Formula weight = 150.09 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.460, non-H atomic volume = 17.1 and following cell contents and analysis: C 20.00 32.01 % H 30.00 4.03 % O 30.00 63.96 % F(000) = 390.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 04mbh0606.ins set up as follows: TITL 04mbh0606 in P-1 CELL 0.71073 4.8651 9.4161 19.1274 98.133 95.126 97.982 ZERR 5.00 0.0021 0.0032 0.0119 0.030 0.069 0.031 LATT 1 SFAC C H O UNIT 20 30 30 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------